Method for detecting residues of eight organic matters in ion exchange resin by adopting headspace gas phase method

A technology of ion exchange resin and headspace gas phase, applied in the field of chemical analysis, to achieve the effect of optimizing chromatographic conditions, good separation, and improving accuracy

Active Publication Date: 2021-02-19
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, there is no official standard for macroporous resin products used in the food industry in my country, but there are some documents that limit individual types of resin products. Purification technology for separation based on the positive and negative charges of the isolates and the difference in charge

Method used

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  • Method for detecting residues of eight organic matters in ion exchange resin by adopting headspace gas phase method
  • Method for detecting residues of eight organic matters in ion exchange resin by adopting headspace gas phase method
  • Method for detecting residues of eight organic matters in ion exchange resin by adopting headspace gas phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Preparation of standard working solution:

[0062] Prepare standard working solution of methyl isopropyl ketone: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,

[0063] Prepare standard working solution of methyl methacrylate: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,

[0064] Prepare 3-pentanone standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200 μg / mL,

[0065] Prepare standard working solution of methyl butyrate: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,

[0066] Prepare 1,2-dichloroethane standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,

[0067] Prepare 1,3-diethylbenzene standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,

[0068] Prepare 1,4-diethylbenzene standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL,

[0069] Prepare m-dichlorobenzene standard working solution: 0.02μg / mL, 0.2μg / mL, 2μg / mL, 20μg / mL, 200μg / mL; the solvents are dimethyl sulfoxide stand...

Embodiment 2

[0090] (1) Optimization of headspace sampler equilibrium temperature:

[0091] On the basis of Example 1, under the condition of other parameters being fixed, samples were injected after equilibrating at constant temperature of 50, 60, 70, and 80°C in the headspace for 30 minutes, and the influence of different equilibrium temperatures on the peak area of ​​the target was investigated.

[0092] See Figure 15 ~ Figure 18 . The results show that in the range of 40-90°C, the peak areas of the eight organic compounds increase with the increase of temperature, and the analysis sensitivity is higher; Condensation, resulting in reduced accuracy and possibly increased interference. Combined with the constant temperature state control performance of the sampler, headspace pressure resistance and tightness and other factors, 80°C was selected as the standard equilibrium temperature.

[0093] (2) Optimization of headspace sampler equilibration time:

[0094] On the basis of Example ...

Embodiment 3

[0097] (1) Selection of chromatographic column:

[0098] When using DB-624 (30m×0.53mm, 1.0μm) quartz capillary column and DB-WAX (30m×0.25mm×0.25μm) quartz capillary column to separate the mixed standard, the 8 kinds of organic substances could not be separated, see Figure 22 ~ Figure 24 , it can be seen that the separation effect of the sample is good when using DB-23 (30m×0.25mm×0.25μm).

[0099] (2) The solvent is replaced by methanol: see the peak results when methanol is used as the solvent Figure 25 , may overlap with the target organism and result in inaccurate results.

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Abstract

The invention discloses a method for detecting residues of eight organic matters in ion exchange resin by adopting a headspace gas phase method, which comprises the following steps of: performing ultrasonic extraction on a sample by using dimethyl sulfoxide by using a chemical analysis technical method, optimizing an extraction method and chromatographic conditions of the sample, and performing baseline separation and statistics on the eight residues; and enabling the linear correlation coefficients in the investigated concentration range to be all 0.999 or above, obtaining the lowest detection limit is obtained. The method is simple, accurate and reliable, and is suitable for determining the organic residual organic solvent in the adsorption resin.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and in particular relates to a method for detecting eight kinds of organic residues in an ion-exchange resin by a headspace gas phase method. Background technique [0002] Ion-exchange chromatography (Ion-exchange chromatography, IEC) has been rapidly promoted in the food and pharmaceutical industries due to its simple process, green environmental protection, and low cost. At the same time, there is currently no official standard for macroporous resin products used in the food industry in my country, but there are some documents that limit individual types of resin products. Purification technology for separation based on the positive and negative charges of the isolates and the difference in charge. . In the food industry, in addition to producing special water supply and treating waste water, it can also be used for desalination, decolorization, separation, purification, and catalysis...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 夏海锋朱贺文臧颖超张光生
Owner JIANGNAN UNIV
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